Beruflich Dokumente
Kultur Dokumente
Sulphatesolubility
Ifasolutionofanysulphateisaddedtoasolutionofagroup2metalcompoundthenaprecipitateislikely.
Group2ioninsolution Effectofaddingasulphatesolution
Mg2+
Noprecipitate,MgSO4issoluble
Ca2+
WhiteprecipitateofCaSO4
Sr2+
WhiteprecipitateofSrSO4
Ba2+
WhiteprecipitateofBaSO4
Hydroxidesolubility
Ifsodiumhydroxideisaddedtoasolutionofagroup2compoundthenaprecipitateislikely.
Group2ioninsolution Effectofaddingahydroxidesolution
Mg2+
FaintwhiteprecipitateofMg(OH) 2
Ca2+
FaintwhiteprecipitateofCa(OH)2
Sr2+
FaintwhiteprecipitateofSr(OH) 2onstanding
Ba2+
Noprecipitate,Ba(OH)2issoluble
Heatingcarbonatesandnitrates
Substance
Effectofheat
Lithiumandallgroup2carbonates Carbondioxidedetected
Sodiumandpotassiumcarbonates
Noeffect(exceptwaterofcrystallisationmaybegiven
off)
Sodiumandpotassiumnitrates
Oxygenonlygasevolved
Lithiumandallgroup2nitrates
Nitrogendioxideandoxygenevolved
Actionofheatoncompounds
CarbonatesCarbondioxideisgivenoff.
HydrogencarbonatesCarbondioxideandwaterformed.
Group1nitratesNitriteandoxygenformed.
Group2nitratesOxide,brownfumesofnitrogendioxideandoxygenformed.
Distinguishingbetweenhydrocarbons
Alkane:Burn/oxidise/combustthem.TheywillburnwithayellowflameandformCO 2 andH2O(limited
supplyofCO).
Alkene:Ayellow,sootierflameisproduced(duetotheextracarbonandhigherratioofcarbon:hydrogen).
Identifyingsomefunctionalgroups
AlkeneAddtoorangebrominewater.Thealkenewilldecolouriseit.
HalogenalkaneHeatwithsodiumhydroxidesolution.Acidifywithdilutenitricacidandthentestwithsilver
nitratesolutionaswithinorganichalides.
AlcoholsorcarboxylicacidscontainingCOHInadrytesttube(i.e.dryalcohol),addPCl 5.Mistyfumesof
HClareproduced,whichturnsbluelitmuspaperred.
Distinguishingbetweendifferentclassesofalcohol
PrimaryAddPCl5.Warmitwithaqueouspotassiumdichromate(K 2Cr2O7)anddiluteH2SO4.Mistyfumesaregiven
offandthecolourchangedfromorangetogreenaldehyde.
SecondaryMistyfumes,changestogreenketone.
TertiaryMistyfumes,nocolourchange.
Specification
f)interpretquantitativeandqualitativeresults
g)deviseandplansimpleexperimentsbasedonthechemistryandtechniquessummarisedinatoeaboveNormally
thelastquestiononthepaper.Itwillaskyoutoidentifycertaincompoundsfromfour.
E.g.titrations,howtomakeastandardsolution,howtotitrate,identifyQCO3whenheatingitwhereQisagroup2
metalion.
h)evaluateerrorinquantitativeexperiments
j)Commentonsafetyaspectsofexperimentsbasedonsupplieddataorrecallofthechemistryofthecompounds
listedinUnitsland2.Safetyconsiderationsshouldrelatetospecificexperimentsnotbeofageneralnatureitwillbe
assumedthatstudentsweareyeprotectionduringallpracticalwork.
Halogensaretoxicandharmfulbyinhalation,althoughiodineismuchlesssothanchlorineorbromine,becauseitisa
solid.Chlorineandbrominemustalwaysbeusedinafumecupboard.Liquidbrominecausesseriousburnsanmustbe
handledwithgloves.
Ammoniaistoxic.Concentratedammoniasolutionsshouldbehandledinthefumecupboard.
Concentratedmineralacidsarecorrosive.Ifspiltonthehands,washingwithplentyofwaterisusuallyenough,but
advicemustbesought.Acidintheeyerequiresimmediateattentionandpromptprofessionalmedicalattention.
Bariumchloridesolutionandchromatesanddichromatesareextremelypoisonousandsoshouldbeusedinthefume
cupboard/shouldnotbeinhaled.
Sodiumorpotassiumhydroxideorconcentratedammoniaintheeyeisextremelyseriousandmustalwaysreceive
professionalandimmediateattention.Sodiumhydroxideandotheralkalimetalhydroxidesareamongstthemost
damagingofallcommonsubstancestoskinandothertissue.Weargloves,gogglesandanapronwhenhandlingthese
solutionsinhighconcentrations.
Generalsafety
Toxic/carcinogenicusegloves,fumecupboard
FlammableWaterbaths,nonakedfumes.
HarmfulgasesUsefumecupboard
Corrosiveweargoggles/gloves
Spillageofconcentratedacidwashwithplentyofwater.
TESTS
Ion
Carbonate
Formula
Test
CO32
Test1
Heatthesolidinatesttubewitha
Bunsenburner.
Observations
Limewatershouldturnfrom
colourlesstocloudyinthepresence
ofcarbondioxidedueto
precipitationofcalciumcarbonate.
Itshoulddecomposeproducingthe
oxideandcarbondioxide.E.g.
CuCO3(s)=CuO(s)+CO2(g)
Testforthegasusinglimewater
solution.
Test2
AdddiluteHCltothesolid.
Testforthegasevolvedusing
Vigorouseffervescence.
Limewatershouldturnfrom
colourlesstocloudyinthepresence
limewatersolution.
ofcarbondioxidedueto
precipitationofcalciumcarbonate.
Hydrogencarbonate
HCO3
Test
Addcalciumchloridetoa
hydrogencarbonatesolution.
Noprecipitateformssincecalcium
hydrogencarbonateissoluble.
Sulphate(VI)
SO42
Test
Addbariumchloridesolution
acidifiedwithdiluteHCltothetest
solution.
Whiteprecipitateofbariumsulphate
forms.
Sulphite
SO32
Test
WarmthesulphitewithdiluteHCl.
Testforgasesusingacidified
potassiumdichromate(VI)solution
(orpaper)
Thesolutionturnsgreen.
Chloride
Cl
Test1
Addconcentratedsulphuricacidto
thesolidchloride.
Whitesteamyacidicfumesareseen
HClfumes.
Test2
Adddilutenitricacidtoasolutionof
achloridetoacidifythesolution.
Thiseliminatesanycarbonatesor
sulphites.
Addsilverchloridetothesolution.
Adddiluteammoniasolution.
Bromide
Br
Test1
Addconcentratedsulphuricacidto
thesolidbromide.
Test2'
Adddilutenitricacidtoasolutionof
abromidetoacidifythesolution.
Thiseliminatesanycarbonatesor
sulphites.
Addsilverchloridetothesolution.
Addconcentratedammoniasolution.
Iodide
WhiteprecipitateofAgClforms.
Soliddissolves.
Steamybrownishacidicfumesare
seen.
CreamprecipitateofAgBrforms.
Soliddissolves.
Test1
Addconcentratedsulphuricacidto
thesolidiodide.
Purpleacidicfumesareseen.The
mixtureturnstoabrownslurry.
Test2
Adddilutenitricacidtoasolutionof
aiodidetoacidifythesolution.This
eliminatesanycarbonatesor
sulphites.
YellowprecipitateofAgIforms.
Addsilverchloridetothesolution.
Solidisinsoluble.
Addconcentratedammoniasolution.
Nitrate
NO3
Test1
Heatsolidnitrate.
Ifgroup1solid(notLi)thenwill
decomposetogivethenitriteand
oxygen.
Allothersolidnitratesdecomposeto
givethemetaloxide,nitrogen
dioxideandoxygen.
Test2
Boilnitratesolutionwith
aluminium/Devardasalloy,in
sodiumhydroxidesolution.
Testvapourwithredlitmuspaper.
Ammonium
Lithium
NH4+
Li+
Test
Warm ammonium compound with
NaOH.
Test vapours immediately using
dampredlitmuspaper.
Oxygengasisevolvedthatwill
relightaglowingsplint.
Browngasisseen(NO2).Oxygen
gasisalsoevolvedandwillrelight
aglowingsplint.
Litmuspaperturnsblueinthe
presenceofammonia.
NH3
turnsthelitmuspaperblue.
Test
DipnichromewireinHCl.
Acarmineredflameisseen.
Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Sodium
Na+
Test
DipnichromewireinHCl.
Dipwireinsolid.
Ayellowflameisseen.
Heatwireincentreofflame.
Observecolourofflame.
Potassium
K+
Test
DipnichromewireinHCl.
Alilacflameisseen.
Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Magnesium
Mg2+
Test
AddNaOHsolutiontothe
Awhitesolidformswhichis
insolubleinexcessNaOH(aq).This
Ca2+
Calcium
magnesiumsolid.
isMg(OH)2(s)
Test
DipnichromewireinHCl.
Abrickredflameisseen.
Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Sr2+
Strontium
Test
DipnichromewireinHCl.
Acrimsonredflameisseen.
Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Ba2+
Barium
Test
DipnichromewireinHCl.
Aapplegreenflameisseen.
Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
TESTS
Name
Formula
Test
Observations
Hydrogen
H2
Ignitegas.
Squeakypopisheard.
Oxygen
O2
Placeaglowingsplintinasampleof
thegas.
Theglowingsplintrelights.
Carbon
dioxide
CO2
Bubblegasthroughlimewater
(saturatedsolutionofcalcium
hydroxide)
Asolutionturnsfromcolourlesstocloudy.A
white(milky)precipitateofcalcium
carbonateformswhichissparinglysoluble.
Ammonia
NH3
Testforgasusingdampredlitmus
paper.
Litmuspaperturnsblue.
Chlorine
Cl2
Test1
Testforgasusingdamplitmuspaper
(redorblue)
Chlorinebleachesthelitmuspapervery
quickly.
Test2
Testforgasusingmoiststarch
iodidepaper.
Thepaperturnsblueblack.
Test3
Passgasthroughasolutionofa
bromide.
Thesolutionturnsfromcolourlesstoorange.
Test4
Passgasthroughasolutionofan
iodide.
Thesolutionturnsfromcolourlesstobrown
(possiblywithablackprecipitate,iodine).
Nitrogen
dioxide
NO2
Notmanytestsforthisgas.
Thegasisbrown.
Sulphur
dioxide
SO2
Test1
Bubblegasthroughasolutionof
potassiumdichromate(VI)dissolved
insulphuricacid.
Thesolutionturnsfromorangetogreen.
Test2
Bubblegasthroughasolutionof
potassiummanganate(VII)dissolved
insulphuricacid.
Thesolutionturnsfrompurpletocolourless.
Volumetricanalysis
Volumetricanalysis(titration)involvesthereactionbetweentwosolutions.Foronesolution,boththevolumeandthe
concentrationareknown;fortheother,thevolumeonlyisknown.Apparatususedincludesaburette,apipetteanda
volumetricflask.
Whatisastandardsolution?
Asolutionforwhichconcentrationisaccuratelyknown.Theconcentrationmayhavebeenfoundbyaprevious
titrationorbyweighingthesoluteandmakingasolutionofknownvolume.Suchasolutionisaprimarystandard
solution.
Howisa250cm3standardsolutionprepared?
Makesurethatthebalanceiscleananddry.Wipeitwithadampcloth.
Placetheweighingbottleonthepanandtarethebalance(i.e.rezeroit)
Takethebottleoffthebalanceandaddsolidtoit.Thisensuresthatnospillagesfallonthepan.
Whenyouhavetherequiredamount,writeitsvaluedownimmediately.
Replaceonbalance,andiftherequiredamountisadded,withdrawthemass.
Washouta250cm3volumetricflaskthreetimesusingpurewater.
Transferthesolidtoa250cm3volumetricflaskusingafunnel,andwashouttheweighingbottleintotheflask
throughthefunnel.
Addabout100cm3ofdistilledwatertotheflask.
Stirthesolutionusingaglassrod.
Washallremainingapparatusincludingtheglassrod,funnelandtransfertherestofthistotheflask.
10
Makeupto250cm3withdistilledwatersothatthebottomofthemeniscusjusttouchesthe250cm3mark.
Stoppertheflask.
Shaketheflaskvigorouslyand/orinverttheflask5or6timestodissolvethesolid.
Concentrationofsolution=massofsolidused/molarmassofsolidx1000/250(unitsmoldm3)
Usingthepipette
Aglassbulbpipettewilldeliverthevolumestatedonitwithinacceptablelimitsonly.
Usingapipettefiller,drawalittleofthesolutiontobeusedintothepipetteandusethistorinsethepipette.
Fillthepipettetoabout23cm3abovethemark.Pipettefillersaredifficulttoadjustaccurately,soquickly
removethefillerandclosethepipettewithyourforefinger(notthumb).Releasethesolutionuntilthebottom
ofthemeniscusisonthemark.
Immediatelytransferthepipettetotheconicalflaskinwhichyouwilldothetitration,andallowthesolution
todispenseundergravity.
Usingtheburette
Makingsurethatthetapisshut,addabout1015cm3oftheappropriatesolutiontotheburetteandrinseitout,
notforgettingtoopenthetapandrinsethejet.
Closethetapandfilltheburette.Asmallfunnelshouldbeusedtoaddthesolutionbutbecarefulnotto
overfillthefunnel.
Removethefunnel,becausetitratingwithafunnelintheburettecanleadtoseriouserrorifadropofliquidin
thefunnelstemfallsintotheburetteduringthetitration.
11
Bringthemeniscusontothescalebyopeningthetaptoallowsolutiontopassthroughtheburette.Thereisno
particularreasontobringthemeniscusexactlytothezeromark.
Makesurethattheburetteisfulltothetipofthejet.
Afterasuitableindicatorhasbeenaddedtothesolutionintheconicalflask,swirltheflaskundertheburette
withonehandwhilstadjustingtheburettetapwithyourotherhand.
Addthesolutionintheburettetotheconicalflaskslowly,swirlingtheflaskallthetime.
Astheendpointisapproached,theindicatorwillchangecolourmoreslowly.Thetitrantshouldbeaddeddrop
bydropneartotheendpoint.
Repeatthetitrationuntilyouhavethreeconcordanttitres,i.e.volumesthataresimilar.Thismeanswithin
0.2cm3orbetterifyouhavebeencareful.Takingthemeanofthreetiresthatdifferby1cm3ormoreisno
guaranteeofanaccurateanswer.
12
Commonindicators
Methylorangeyellowinalkali,redinacid(orangeatendpoint)
Phenolphthaleinpinkinalkali,colourlessinacid.
Enthalpychangemeasurements
Weighaspiritlamp(containingaliquidalcohol)usingabalanceaccurateto3decimalplaces.Recordthe
massmeasured.
Useameasuringcylindertoput100cm3ofdistilledwaterintoasmallbeakerandclampsthisatafixed
heightabovethespiritlamp(about2cm).
Recordtheinitialtemperatureofthewaterusingathermometer.
Lightthelampusingaburningsplint.
Heatthewaterusingthespiritlampuntilthetemperaturehasgoneupbyabout10C.Stirthewaterwiththe
thermometerthewholetime.
Putacaponthespirittostopthealcoholburning.Thelidstopsalsostopsfurtherevaporationoftheliquid
alcohol.
Reweighthespiritlampandrecordthemass.
Calculatetheenthalpychange
Possiblesourcesoferror
13
Theremaybeheatlossduetotheapparatususedandheatmayhavedissipatedthroughtheinsulatingmaterial
shoulduseapolystyrenecupandinsulationlikealid.
Thespecificheatcapacityanddensityofwaterareused(andnotofHCl).
Themassesofsolidaddedtotheacidareignored.
Itisassumedthatthespecificheatcapacityofthepolystyrenecupisnegligible.
Someheatislostwhenthehydrogenorcarbondioxideareevolvedinthereactions.
Manyorganicreactionsareslowandrequireprolongedheating
Toachievethiswithoutlossofliquid,reactionmixturesareheatedinaflaskcarryingaverticalcondenser.
Thisisheatingunderreflux;thesolventiscondensedandreturnedtotheflask,sothemixturecanbeheated
aslongasdesired.
Toheattheroundbottomedflask,eitheruseawaterbath,anoilbathoraheatedplatemantle.ABunsen
burnerisntreallysuitable.
Simpledistillation
Toseparateavolatilesolventfromamixture
Simpledistillationisusedwhereavolatilecomponenthastobeseparatedfromamixture,theother
componentsofthemixturebeingverymuchvolatileornonvolatile.
Themixtureisheated.
Thefractionthatboilsiscollectedwithinthetemperaturerangeofthefraction.(normally1or2degrees
beforetheboilingtemperature)
Thecondensercoolsthefractionsoitdistilsandiscollectedinthereceivingflask.
14
Fractionaldistillation
Toseparatemixturesofvolatileliquids.
RecrystallisationUsedtopurifyasolidmaterialbyremovingbothsolubleandinsolubleimpurities.The
choiceofsolventisimportant.Thesubstancemustbeeasilysolubleintheboilingsolventandmuchless
soluble at room temperature. This ensures the smallest possible loss of material, although some loss is
inevitablewiththistechnique.
Recrystallisationmethod
1. Dissolvethesolidintheminimumamountofboilingsolvent.Thisensuresthatthesolutionissaturatedwith
respecttothemainsolutebutnotwithrespecttotheimpurities,whicharepresentinmuchsmalleramounts.
2. Filterthehotmixturethroughapreheatedfilterfunnel.Thisremovesinsolubleimpurities.Thehotfunnelis
necessarytopreventthesolutecrystallisingandblockingthefunnel.Filtrationundervacuumusinga
Buchnerfunnelisoftenpreferred,becauseitisfast.
3. Coolthehotfiltrate,eithertoroomtemperatureor,ifnecessary,inabathoficedwater.Rapidcoolinggives
smallcrystals,slowcoolinglargeones.Thelargecrystalsareoftenlesspure.
4. FilterthecoldmixtureusingaBuchnerfunnel.
5. Washthecrystalswithasmallamountofcoldsolvent.Thisremovesanyimpurityremainingonthesurfaceof
thecrystals.Asmallamountofcoldsolventisusedsothatthecrystalsarentwashedaway/dontdissolve.
6. Suckthecrystalsasdryaspossibleonthefilter.
7. Transferthecrystalstoadesiccatortodry.Dryingbetweenfilterpaperissometimesrecommended,butitisa
verypoormethod.
15
16
Meltingpointdetermination
Thisisusedtodeterminethepurityoftherecrystallisationsolid.Placesmallamountofthesolidinthesealedendof
acapillarytube.Placeinthemeltingpointapparatus.Asharpmeltingpointoverasmallrangeshowspurity,when
comparedwiththesetbookvalueofahighermeltingpoint,thatindicatesanimpuresolid.
17
Organictests
Collect10cmofthesamples.
Testthesamplesinthefollowingorder
Alkenesbrominewaterdecolourisesalkene
AlcoholsSpatulaofsolidPCl5.Testfumeswithdamplitmuspaperlitmusred?Whitefumesnear
ammonia?alcohol
HalogenoalkaneAddNaOH,ethanolassolvent.Shakeandwarmfor3minutes.Coolandaddnitricacid+
silvernitrate.white=chloride;cream=bromide;yellow=iodide.Confirmwithammonia
Alkane,thesubstanceleftisthealkane.
18